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Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish

文献类型： 外文期刊

作者： Yang, Xianli 1 ; Zhou, Lei 2 ; Tan, Yanglan 3 ; Shi, Xizhi 2 ; Zhao, Zhiyong 1 ; Nie, Dongxia 1 ; Zhou, Changyan 1 ; Liu, 1 ;

作者机构： 1.Shanghai Acad Agr Sci, Inst Agrofood Stand & Testing Technol, Lab Qual & Safety Risk Assessment Agroprod Shangh, Minist Agr, Shanghai 201403, Peoples R China

2.Ningbo Univ, Sch Marine Sci, Ningbo 315211, Zhejiang, Peoples R China

3.Chinese Acad Sci, Shanghai Inst Biol Sci, Inst Nutr Sci, Key Lab Food Safety Res, Shanghai 200031, Peoples R China

4.Shanghai Municipal Ctr Dis Control & Prevent, Shanghai 200336, Peoples R China

关键词： paralytic shellfish poisoning (PSP) toxins;LC-MS/MS;dispersive solid-phase extraction (dSPE);saxitoxin

期刊名称：TOXINS （ 影响因子：4.546； 五年影响因子：4.8 ）

ISSN： 2072-6651

年卷期： 2017 年 9 卷 7 期

页码：

收录情况： SCI

摘要： In this study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) method was developed for simultaneous determination of eight paralytic shellfish poisoning (PSP) toxins, including saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins (GTX1-4) and the N-sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80: 20, v/v) with 0.1% formic and purified by dispersive solid-phase extraction (dSPE) with C18 silica and acidic alumina. Qualitative and quantitative detection for the target toxins were conducted under the multiple reaction monitoring (MRM) mode by using the positive electrospray ionization (ESI) mode after chromatographic separation on a TSK-gel Amide-80 HILIC column with water and acetonitrile. Matrix-matched calibration was used to compensate for matrix effects. The established method was further validated by determining the linearity (R-2 >= 0.9900), average recovery (81.52-116.50%), sensitivity (limits of detection (LODs): 0.33-5.52 mu g.kg(-1); limits of quantitation (LOQs): 1.32-11.29 mu g.kg(-1)) and precision (relative standard deviation (RSD) <= 19.10%). The application of this proposed approach to thirty shellfish samples proved its desirable performance and sufficient capability for simultaneous determination of multiclass PSP toxins in sea foods.

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